Methylprednisolone detection in urine following local and oral administrations

Size: px
Start display at page:

Download "Methylprednisolone detection in urine following local and oral administrations"

Transcription

1

2 Susana MS Simões, Marta Calçada, Luís Horta, Xavier de la Torre Methylprednisolone detection in urine following local and oral administrations Laboratório de Análises e Dopagem. Instituto do Desporto de Portugal. Av. Prof. Egas Moniz (Estádio Universitário). 6-9 LISBOA. Portugal Introduction Glucocorticosteroids are prohibited when administered orally, rectally, intravenously or intramuscularly. In order to investigate the possibility to distinguish between permitted vs an illicit administration of these substances, we conducted two excretion studies after controlled administrations of methylprednisolone through oral and local administrations. Mehylprednisolone urinary detection as well as the effects on the normal endogenous glucocorticosteroids (cortisol and cortisone) excretion were monitored by routine LC/MS/MS analyses after automatic SPE extraction. Experimental Samples obtained after controlled administrations of methylprednisolone were analyzed following the screening and confirmation procedures for methylprednisolone detection. A brief description of the method used is presented in Figure. Methylprednisolone, methylprednisone, 2α-hydroxymethylprednisolone (see Figure 2), cortisol and cortisone were monitored. Cortisol and cortisone were compared with population based data obtained from routine samples of the Portuguese doping control program. Oral administration: 4 mg of methylprednisolone (Medrol, Pfizer) were given orally to a male volunteer. Local administration: Samples were collected from an athlete (that had a TUE accepted by the National Portuguese Antidoping Council (CNAD). 4 mg of Depo-Medrol, Pfizer by extraarticular infiltation) that volunteered for the study. 4

3 Results After both administrations, concentrations higher than the reporting threshold (3 ng/ml) proposed by WADA are reached (c.a. h for the oral administration and 36 h for the local one) with slightly higher peak concentration after the local administration. Methylprednisolone can be detected up to 32 h after oral administration and 8 h after local administration. The excretion profile of the 3 metabolites monitored is similar. The relative response of 2α-hydroxymethylprednisolone is in both administrations higher than methylprednisolone itself being a more sensitive marker of methylprednisolone intake. After both administrations a deep suppression of cortisol and cortisone concentrations is observed. The lowest concentrations are below the 5 percentile of the population based data (Figures 3-4 and Table ) reflecting the systemic effect reached in both cases. Conclusions After both oral and local administrations, a systemic effect is observed through the inhibition of the endogenous excretion of cortisol and cortisone. The concentrations reached in the permitted administration (dosage s the oral administration) were higher than after an oral administration. The urinary excretion profile of methylprednisolone and its metabolites is similar in both administrations do not permitting to differentiate the route of administration. Figure. Description of the method used. 3 ml of urine Add.3 µg of methyltestosterone (internal standard) ml of sodium acetate buffer.2 M ph 5.2 and 5 µl of β-glucuronidase/ arylsulfatase Incubate the samples at 55ºC for 2 h Condition the Oasis HLB columns with 3 ml of methanol and 3 ml of water Load 4 ml of the samples into the columns Wash the columns with 3 ml of sodium hydroxide.2m: methanol (6:4, v/v) and 3 ml of water Elute the samples with 3 ml of tert-butylmethyl ether: methanol (9:, v/v) Evaporate to dryness under nitrogen at 45 C. Reconstitute in µl of mobile phase Transfer the mixture to a 2 µl vial, and analyse the sample by LC/MS/MS Instrument Waters Alliance 2795 pump/ Micromass Quattro micro TM Column Waters-XTerra MS C8 (5 mm, 2. mm, 5 µm) Flow parameters solvent A ACN/HCOOH. (95:5) solvent B HCOOH./ACN (95:5) flow rate.3 ml/min 65 Mass spectrometric parameters acquisition mode MRM function -6.5 min ( ) cone 2V coll 5eV ( ) cone 2V coll 5eV ( ) cone 2V coll 5eV function min ( ) cone 2V coll 5eV ( ) cone 2V coll 5eV ( ) cone 2V coll 5eV ( ) cone 2V coll ev ( ) cone 2V coll ev ( ) cone 2V coll ev function 2-6 min ( ) cone 35V coll 22eV ( ) cone 35V coll 22eV 42

4 Figure 2. LC/MS/MS analysis of a urine sample collected c.a. 2 h after the infiltration I. 375>357; 375>339 Methylprednisolone II. 373>355; 373>337 Methylprednisone III. 377>28; 377>359-2α-Hydroxymethylprednisolone III I II > e > e > e > e > e > e Time Table. Non-parametric data of population distribution of cortisol and cortisone in routine samples (n=82) 5 Median Mean 95 Cortisol (ng/ml) Cortisone (ng/ml) (5, 95: percentiles) 43

5 Figure 3. Relative urinary detection of methylprednisolone and metabolites after oral and local administrations Oral (4mg) Infiltration (4mg) Metilprednisolona Metilprednisona (met.) 2a-Hidroximetilprednisolona (met.) 6 4 Metilprednisolona Metilprednisona (met.) 2a-Hidroximetilprednisolona (met.) A/A(IS)* 25 2 A/A(IS)* Figure 4. Urinary methylprednisolone and effect on the HPA axis after oral and local administrations Conc. (ng/ml) Methylprednisolone Oral 4 mg (p.o.) Methylprednisolone Hydrocortisone Cortisone Conc. (ng/ml) Methylprednisolone Infiltration 4mg Methylprednisolone Hydrocortisone Cortisone 44

Simultaneous Determination of a Panel of 22 Steroids in Urine and Serum by SPE and LC-MS/MS

Simultaneous Determination of a Panel of 22 Steroids in Urine and Serum by SPE and LC-MS/MS Simultaneous Determination of a Panel of 22 Steroids in Urine and Serum by SPE and LC-MS/MS UCT Part Numbers: CUQAX22Z Clean-Up C8+QAX, 2mg/1mL BETA-GLUC- ml Beta-Glucuronidase Enzyme, liquid form SLAQID21-3UM

More information

May 1, By John Heim,Doug Staples

May 1, By John Heim,Doug Staples 1 of 7 7/11/2014 3:39 PM May 1, 2010 By John Heim,Doug Staples Anabolic steroid screening analysis in urine is complex and labor intensive requiring sensitive instrumentation and optimized chromatographic

More information

Trace-Level Analysis of Metanephrines in Plasma by HILIC LC-MS/MS

Trace-Level Analysis of Metanephrines in Plasma by HILIC LC-MS/MS Abstract Highly sensitive analysis of metanephrines in plasma is critical in the diagnosis and treatment of pheochromocytoma and paraganglioma. Here, a HILIC LC-MS/MS method was developed using a Raptor

More information

High speed UHPLC-MS/MS determination of multiple steroids in human serum using the Nexera MX system for multiplex analysis

High speed UHPLC-MS/MS determination of multiple steroids in human serum using the Nexera MX system for multiplex analysis PO-CON695E High speed UHPLC-MS/MS determination of multiple steroids in human serum using the Nexera MX system for multiplex analysis MSACL 6 EU Neil Loftus, Stephane Moreau, Mikaël Levi 3, Anja Grüning

More information

WADA Technical Document TD2014EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting

WADA Technical Document TD2014EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting Endogenous Anabolic Androgenic Steroids Measurement and Reporting 1.0 Introduction The purpose of this Technical is to harmonize the approaches to the measurement and reporting of endogenous anabolic androgenic

More information

Longterm Detection of Anabolic Steroid Metabolites in Urine

Longterm Detection of Anabolic Steroid Metabolites in Urine Longterm Detection of Anabolic Steroid Metabolites in Urine Application Note Forensics/Doping Control Author Stephan Baumann Agilent Technologies, Inc. 5301 Stevens Creek Blvd Santa Clara, CA 95051 USA

More information

Extend the time window for the detection of low level anabolic androgenic steroids and their metabolites

Extend the time window for the detection of low level anabolic androgenic steroids and their metabolites Application Note Doping Control Extend the time window for the detection of low level anabolic androgenic steroids and their metabolites Steroid profiling, screening, and confirmatory analysis using the

More information

Integration of amino acid, acylcarnitine and steroids analysis in single FIA/LC-MS/MS platform

Integration of amino acid, acylcarnitine and steroids analysis in single FIA/LC-MS/MS platform POCON3E Integration of amino acid, acylcarnitine and steroids analysis in single FIA/LCMS/MS platform ASMS 2 ThP2 Tetsuo Tanigawa, Toshikazu Minohata Shimadzu Corporation, Kyoto, Japan analysis in single

More information

WADA Technical Document TD2016EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting

WADA Technical Document TD2016EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting Endogenous Anabolic Androgenic Steroids Measurement and Reporting Introduction The purpose of this Technical Document (TD) is to harmonize the approaches to the measurement and reporting of Endogenous

More information

1. INTRODUCTION CH 3 CH3

1. INTRODUCTION CH 3 CH3 1. ITRODUCTIO TITLE: Analysis of stanozolol and metabolites S.O.P. : ARO/446 in urine Page : 1 of 12 This method describes the analysis of stanozolol, 4ß-hydroxy-stanozolol and 16ß-hydroxy-stanozolol in

More information

Hair analyses. Hair analysis beyond workplace testing. Ia: Fatal steroid abuse. Identification of stanozolol in hair

Hair analyses. Hair analysis beyond workplace testing. Ia: Fatal steroid abuse. Identification of stanozolol in hair Hair analyses Hair analysis beyond workplace testing Detlef Thieme IDAS Kreischa IRM + FTC Munich. anabolic (steroids, clenbuterol). kinetic (segmentation and profiling) 3. genetic (amitriptyline vs.nortriptyline

More information

Introduction. Experimental

Introduction. Experimental PO-CON162E Development of Automated Screening and Quantitation Approach on Novel On-Line SFE-SFC-MS/MS Platform (I) For 23 Restricted Perflurocompounds in Textiles ASMS 2016 MP 283 Jie Xing, Jun Xiang

More information

Renzo BAGNATI Mario Negri Institute of Pharmacological Research- IRCCS Milano - Italy

Renzo BAGNATI Mario Negri Institute of Pharmacological Research- IRCCS Milano - Italy STEROIDS IN WASTE WATERS AS MARKERS OF ABUSE Renzo BAGNATI Mario Negri Institute of Pharmacological Research- IRCCS Milano - Italy A first attempttoapplythe sewage epidemiologyapproachin doping Compare

More information

WADA Technical Document TD2018MRPL

WADA Technical Document TD2018MRPL MINIMUM REQUIRED PERFORMANCE LEVELS FOR DETECTION AND IDENTIFICATION OF NON-THRESHOLD SUBSTANCES In order to ensure that all WADA-accredited Laboratories can report the presence of Prohibited Substances,

More information

WADA Technical Document TD2017NA

WADA Technical Document TD2017NA HARMONIZATION OF ANALYSIS AND REPORTING OF 19-NORSTEROIDS RELATED TO NANDROLONE 1.0 Introduction This document has been established to harmonize the Confirmation Procedure for the analysis and reporting

More information

SOP: Derivatized testosterone_01 Revision: 01 Date Effective: 05/17/15

SOP: Derivatized testosterone_01 Revision: 01 Date Effective: 05/17/15 Chemicals needed: Precipitate solution, Methanol Derivatization Solution, Amplifex Keto Reagent Kit Mobile phases, H 2 0 with 0.1% Formic Acid LC/MS grade and Acetonitrile with 0.1% Formic Acid LC/MS grade

More information

The Application of QuEChERS in the Extraction of Anabolic Steroids in Whole Blood

The Application of QuEChERS in the Extraction of Anabolic Steroids in Whole Blood The Application of QuEChERS in the Extraction of Anabolic Steroids in Whole Blood UCT Part Numbers: ECQUUS1015CT- Enviro-Clean 15 ml centrifuge tube with 400 mg MgSO 4 and 100 mg NaCl CUMPS2CT - Enviro-Clean

More information

SPECIFIC DETECTION OF ANDROST-4-ENE-3,17-DIONE

SPECIFIC DETECTION OF ANDROST-4-ENE-3,17-DIONE 7 SPECIFIC DETECTION OF ANDROST-4-ENE-3,17-DIONE ADMINISTRATION BY PROFILING OXYGENATED METABOLITES Abstract For the selective detection of androst-4-ene-3,17-dione ( 4-AEDIONE) administration, the analysis

More information

SCREENING OF TRENBOLONE-17β IN MILK SAMPLES AFTER APPLICATION OF TRENBOLONE ACETATE TO A CULL COW

SCREENING OF TRENBOLONE-17β IN MILK SAMPLES AFTER APPLICATION OF TRENBOLONE ACETATE TO A CULL COW SCREENING OF TRENBOLONE-17β IN MILK SAMPLES AFTER APPLICATION OF TRENBOLONE ACETATE TO A CULL COW Iris G. Lange, Andreas Daxenberger, Heinrich H. D. Meyer Institut für Physiologie, Forschungszentrum für

More information

Automated Low Background Solid Phase Extraction of Perfluorinated Compounds in Water. Ruud Addink Fluid Management Systems Watertown MA

Automated Low Background Solid Phase Extraction of Perfluorinated Compounds in Water. Ruud Addink Fluid Management Systems Watertown MA Automated Low Background Solid Phase Extraction of Perfluorinated Compounds in Water Ruud Addink Fluid Management Systems Watertown MA Introduction Perfluoralkylated compounds contain a perfluorinated

More information

User guide for operating the Agilent 6420A QqQ mass spectrometer by direct infusion/injection

User guide for operating the Agilent 6420A QqQ mass spectrometer by direct infusion/injection User guide for operating the Agilent 6420A QqQ mass spectrometer by direct infusion/injection This user guide does not have the intention to introduce you to any of the theory and/or principles behind

More information

Hair Testing to provide additional evidence in doping cases of potential (clenbuterol) contaminations

Hair Testing to provide additional evidence in doping cases of potential (clenbuterol) contaminations Hair Testing to provide additional evidence in doping cases of potential (clenbuterol) contaminations Detlef Thieme Institute of Doping Analysis, Dresden, Germany Beijing, Oct 2017 [M. Jahn (www.kreischa.net)]

More information

extraction of EG and DEG from the matrix. However, the addition of all diluent at once resulted in poor recoveries.

extraction of EG and DEG from the matrix. However, the addition of all diluent at once resulted in poor recoveries. Informal Commentary Limit of Diethylene Glycol (DEG) and Ethylene Glycol (EG) in Sorbitol Solution, Sorbitol Sorbitan Solution and Noncrystallizing Sorbitol Solution December 2009 Monograph/Section(s):

More information

Development of a Clinical Research Method for the Measurement of Testosterone. Dihydrotestosterone

Development of a Clinical Research Method for the Measurement of Testosterone. Dihydrotestosterone Development of a Clinical Research Method for the Measurement of Testosterone and Dihydrotestosterone Martijn van Faassen, Maarten van den Noort and Ido Kima University Medical Center, Groningen, Netherlands

More information

Dissolution test results showing biorelevant media made from SIF Powder Original is the same as media prepared using methylene chloride

Dissolution test results showing biorelevant media made from SIF Powder Original is the same as media prepared using methylene chloride Dissolution test results showing biorelevant media made from SIF Powder Original is the same as media prepared using methylene chloride Michael Schaich, Bastian Kloefer, Mathew Leigh : info@biorelevant.com

More information

Extended Application Note

Extended Application Note Extended Application Note Harmful Substances in Dietary Supplements HPLC Columns with APP A-337 www.mtc-usa.com 1-732-578-1777 INTRODUCTION A dietary supplement is a substance to be consumed for the purpose

More information

WADA Technical Document TD2018EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting

WADA Technical Document TD2018EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting Endogenous Anabolic Androgenic Steroids Measurement and Reporting 1.0 Introduction The purpose of this Technical Document (TD) is to harmonize the approaches to the measurement and reporting of Endogenous

More information

GCMSD-Headspace Analysis SOP

GCMSD-Headspace Analysis SOP Before you start GCMSD-Headspace Analysis SOP Method and Sequences names are restricted to 50 characters (MSD program will crash otherwise) The GC oven and Injection Ports need to be cooled to 50 oc to

More information

MV5: Automated concentration system

MV5: Automated concentration system MV5: Automated concentration system Abstract LabTech MV5 is the latest automatic nitrogen evaporator developed by our R&D Team able to process up to 54 samples simultaneously. This advanced instrument

More information

A NOVEL RP-HPLC METHOD FOR THE QUANTIFICATION OF ICATIBANT IN FORMULATIONS

A NOVEL RP-HPLC METHOD FOR THE QUANTIFICATION OF ICATIBANT IN FORMULATIONS A NOVEL RP-HPLC METHOD FOR THE QUANTIFICATION OF ICATIBANT IN FORMULATIONS B.Lakshmi,Kallam Haranadhareddy Institute of Technology, Guntur Prof T.V.Reddy,Prof Mallareddy College of Engineering, Secunderabad

More information

OMCL Network of the Council of Europe QUALITY ASSURANCE DOCUMENT

OMCL Network of the Council of Europe QUALITY ASSURANCE DOCUMENT OMCL Network of the Council of Europe QUALITY ASSURANCE DOCUMENT PA/PH/OMCL (16) 17 R QUALIFICATION OF EQUIPMENT ANNEX 2: QUALIFICATION OF GC EQUIPMENT Full document title and reference Document type Legislative

More information

Toxicology Gas Chromatography-Mass Spectrometry (GC-MS)

Toxicology Gas Chromatography-Mass Spectrometry (GC-MS) Toxicology Gas Chromatography-Mass Spectrometry (GC-MS) 1.0 Purpose - This procedure specifies the required elements for the calibration and use of the Agilent Gas Chromatograph interfaced to the Agilent

More information

TRACE LEVEL DETERMINATION OF PER- AND POLYFLUOROALKYL SUBSTANCES (PFASs) IN WATER USING THE AGILENT 6460 LC/MS/MS

TRACE LEVEL DETERMINATION OF PER- AND POLYFLUOROALKYL SUBSTANCES (PFASs) IN WATER USING THE AGILENT 6460 LC/MS/MS ENVIRONMENTAL MARKET TRACE LEVEL DETERMINATION OF PER- AND POLYFLUOROALKYL SUBSTANCES (PFASs) IN WATER USING THE AGILENT 6460 LC/MS/MS A method for the determination of per- and polyfluoroalkyl substances

More information

Sample purification procedure for confirmation of 3 -hydroxy stanozolol by gas chromatography/high resolution mass spectrometry

Sample purification procedure for confirmation of 3 -hydroxy stanozolol by gas chromatography/high resolution mass spectrometry Author proof done Research Article Sample purification procedure for confirmation of 3 -hydroxy stanozolol by gas chromatography/high resolution mass spectrometry S. Ahi, I. M. Reddy, A. Beotra, R. Lal,

More information

Monitoring Hormone Therapy Mark Newman, M.S. President of Precision Analytical Inc.

Monitoring Hormone Therapy Mark Newman, M.S. President of Precision Analytical Inc. Mr Mark Newman Monitoring Hormone Therapy Mark Newman, M.S. President of Precision Analytical Inc. 2 Avoiding Pitfalls in (B)HRT Monitoring and Picking the Right Lab Test Objectives: Outline how expected

More information

Evaluation of linear and step gradient performance and retention time precision of the Agilent 1200 Series Rapid Resolution LC

Evaluation of linear and step gradient performance and retention time precision of the Agilent 1200 Series Rapid Resolution LC Evaluation of linear and step gradient performance and retention time precision of the Agilent 12 Series Rapid Resolution LC This document is believed to be accurate and up-to-date. However, Agilent Technologies,

More information

Technical Procedure for Drug Chemistry Gas Chromatograph/Mass Spectrometry (GC-MS)

Technical Procedure for Drug Chemistry Gas Chromatograph/Mass Spectrometry (GC-MS) Technical Procedure for Drug Chemistry Gas Chromatograph/Mass Spectrometry (GC-MS) 1.0 Purpose - This procedure specifies the required elements for the calibration and use of the Agilent 6890 GC interfaced

More information

The instrument should have a mass range from 2 to 2000 m/z or better Interface

The instrument should have a mass range from 2 to 2000 m/z or better Interface Revised Specifications for Liquid Chromatography Mass Spectrometry (LC-MS/MS ) Triple Quadrupole Specification for Ultra-Fast Liquid Chromatography system Solvent Delivery 1) A quaternary Pump system for

More information

Beyond Analytical Results

Beyond Analytical Results WADA / Science and Investigations Symposium - Istanbul Beyond Analytical Results Martial Saugy, Norbert Baume, Neil Robinson, Nicolas Jan, François Marclay Swiss Laboratory for Doping Analyses Centre Hospitalier

More information

(2 pts) Draw the line of best fit through the data and estimate the concentration of Fe in your sample solution.

(2 pts) Draw the line of best fit through the data and estimate the concentration of Fe in your sample solution. Name: 1. You are asked to measure the percent iron in a steel sample you believe to be about 50% Fe by mass. You dissolve four replicate samples in nitric acid and dilute them by mass to a concentration

More information

A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples

A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples Research Article A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples I. Madhusudhana Reddy, Alka Beotra, S. Jain, S. Ahi ABSTRACT National Dope Testing Laboratory,

More information

Studies on the determination of chlorotestosterone and its metabolites in bovine urine

Studies on the determination of chlorotestosterone and its metabolites in bovine urine Studies on the determination of chlorotestosterone and its metabolites in bovine urine Michaela Walshe, a Michael Keeffe a and Bruno Le Bizec b a Teagasc, The National Food Centre, Dunsinea, Castleknock,

More information

EVALUATION OF PROFICIENCY TESTING PROGRAM, SETTING PRIORITIES FOR THE FUTURE.

EVALUATION OF PROFICIENCY TESTING PROGRAM, SETTING PRIORITIES FOR THE FUTURE. Click to edit Master title style EVALUATION OF PROFICIENCY TESTING PROGRAM, SETTING PRIORITIES FOR THE FUTURE. Saskia S. Sterk Henk A. Herbold, Marco H. Blokland October 2005. Introduction. One of the

More information

USER'S GUIDE. Nanoflow Probe. Red Stripe. 3-4mm. ptfe Sleeve. To Injector. ZU1XC Fused Silica TTF115. Fused Silica. ptfe Sleeve

USER'S GUIDE. Nanoflow Probe. Red Stripe. 3-4mm. ptfe Sleeve. To Injector. ZU1XC Fused Silica TTF115. Fused Silica. ptfe Sleeve USER'S GUIDE Nanoflow Probe 3-4mm Red Stripe ptfe Sleeve To Injector ZU1XC Fused Silica 20µm 90µm TTF115 ptfe Sleeve Fused Silica 25µm 375µm Micromass UK Limited Floats Road Wythenshawe M23 9LZ Tel: +44

More information

Member Federations Council and Commission Members. Circular No 3 of 2017 Anti-Doping Programme Information

Member Federations Council and Commission Members. Circular No 3 of 2017 Anti-Doping Programme Information Lausanne, Switzerland To: Member Federations Council and Commission Members Circular No 3 of 2017 Anti-Doping Programme Information Ladies and Gentlemen, Anti-Doping Obligations for Rowers and National

More information

UWW ANTI-DOPING PANEL DECISION. Case

UWW ANTI-DOPING PANEL DECISION. Case UWW ANTI-DOPING PANEL DECISION Case United World Wrestling (UWW) v. Mr Husham Majeed Ali AL THAALEBI (Athlete GR wrestling member of the Iraqi national team) Panel: - Dr Daniel Wozniak - Dr Milica Vukasinovic-Vesic

More information

Automated Determination of Dissolved Gases in Water By Headspace Calibration of Mixed Gases Anne Jurek

Automated Determination of Dissolved Gases in Water By Headspace Calibration of Mixed Gases Anne Jurek Automated Determination of Dissolved Gases in Water By Headspace Calibration of Mixed Gases Anne Jurek Abstract: Due to the expansion of natural gas drilling through horizontal fracturing, there has been

More information

PFC Analysis Kit for ACQUITY UPLC System Guide

PFC Analysis Kit for ACQUITY UPLC System Guide PFC Analysis Kit for ACQUITY UPLC System Guide 71500183002/Revision A Copyright Waters Corporation 2009 All rights reserved Copyright notice 2009 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF AMERICA

More information

CHAPTER 10 Reconstitution of Powdered Drugs

CHAPTER 10 Reconstitution of Powdered Drugs CHAPTER 10 RECONSTITUTION OF POWDERED DRUGS 89 CHAPTER 10 Reconstitution of Powdered Drugs Objectives The learner will: 1. prepare solutions from powdered drugs using directions printed on vial labels.

More information

Simplified Backflush Using Agilent 6890 GC Post Run Command Application Note

Simplified Backflush Using Agilent 6890 GC Post Run Command Application Note Simplified Backflush Using Agilent 6890 GC Post Run Command Application Note Gas Chromatography Author Matthew S. Klee Agilent Technologies 2850 Centerville Road Wilmington, DE 19808-1610 USA Abstract

More information

UWPR. LC-MS setup. Before you connect your trap and column. Connecting your trap and column

UWPR. LC-MS setup. Before you connect your trap and column. Connecting your trap and column Before you connect your trap and column You need to provide your own trap and column (Note our fittings accommodate trap and column made with fused silica 360 µm OD). Check our guide for packing traps

More information

SIMPLE, EFFICIENT AND SIMULTANEOUS DETERMINATION OF ANABOLIC STEROIDS IN HUMAN URINE

SIMPLE, EFFICIENT AND SIMULTANEOUS DETERMINATION OF ANABOLIC STEROIDS IN HUMAN URINE SIMPLE, EFFICIENT AND SIMULTANEOUS DETERMINATION OF ANABOLIC STEROIDS IN HUMAN URINE Pages with reference to book, From 216 To 218 S.J. Khurshid, M. Riaz, S. Ahmed ( Nuclear Chemistry Division, Pakistan

More information

Analysis of Casein and Whey Protein in Whole, 2%, and Skim Milk by Capillary Gel Electrophoresis

Analysis of Casein and Whey Protein in Whole, 2%, and Skim Milk by Capillary Gel Electrophoresis Analysis of Casein and Whey Protein in Whole, 2%, and Skim Milk by Capillary Gel Electrophoresis Marcia Santos, Staff Applications Scientist, Beckman Coulter Life Sciences, Brea, CA USA Mark Lies, Marketing

More information

All you need to know about anti-doping. Representatives from Hong Kong Anti-Doping Committee

All you need to know about anti-doping. Representatives from Hong Kong Anti-Doping Committee All you need to know about anti-doping Representatives from Hong Kong Anti-Doping Committee Anti-Doping Rule Violations What is DOPING? The occurrence of one or more of the anti-doping rule violations

More information

Automated Determination of Dissolved Gases in Water Anne Jurek. Abstract: Discussion:

Automated Determination of Dissolved Gases in Water Anne Jurek. Abstract: Discussion: Automated Determination of Dissolved Gases in Water Anne Jurek Abstract: The RSK-175 standard operating procedure was developed in order to determine the amount of dissolved gas in water. Due to the expansion

More information

Analysis of Melamine and Cyanuric Acid in Food Matrices by LC-MS/MS

Analysis of Melamine and Cyanuric Acid in Food Matrices by LC-MS/MS Application Note: Analysis of and Cyanuric Acid in Food Matrices by LC-MS/MS PeterVarelis, National Center for Food Safety and Technology, Illinois Institute of Technology. Jonathan Beck, Kefei Wang, and

More information

Chemical Analysis for Methyltestosterone

Chemical Analysis for Methyltestosterone APPLIED CONSUMER SERVICES, INC. Chemical Analysis for Methyltestosterone Report #: 27584 Report to: Mr. Mitch Ross 24 Dockside Lane # 131 Key Largo, Florida 33017 2016 1 1 8 9 0 N W 8 7 t h C o u r t,

More information

GC-MS(/MS) investigations on long-term metabolites of 17-methyl steroids

GC-MS(/MS) investigations on long-term metabolites of 17-methyl steroids M.K. Parr 1), G. Fußhöller 1), M. Gütschow 2), C. Hess 1,2), W. Schänzer 1) GC-MS(/MS) investigations on long-term metabolites of 17-methyl steroids 1) Institute of Biochemistry, German Sport University,

More information

WADA Technical Document TD2010EAAS. Endogenous Anabolic Androgenic Steroids Testing, Reporting and Interpretive Guidance

WADA Technical Document TD2010EAAS. Endogenous Anabolic Androgenic Steroids Testing, Reporting and Interpretive Guidance Endogenous Anabolic Androgenic Steroids Testing, Reporting and Interpretive Guidance 1.0 Introduction The purpose of this Technical Document is to further harmonize the approaches to the detection and

More information

FROG-4000 TM Chemical Analysis System

FROG-4000 TM Chemical Analysis System FROG-4000 TM Chemical Analysis System User s Manual Defiant Technologies, Inc. 2015 Vol.5 This page is intentionally left blank. FROG-4000 TM Chemical Analysis System User s Manual Defiant Technologies,

More information

Validation of the MRM pesticides from the Working Document SANCO/12745/2013 of November 2017 rev. 9(1)

Validation of the MRM pesticides from the Working Document SANCO/12745/2013 of November 2017 rev. 9(1) Validation of the MRM pesticides from the Working Document SANCO/12745/2013 of 21-22 November 2017 rev. 9(1) CONTENTS 1. Aim and scope... 2 2. Short description... 2 3. Apparatus and consumables... 2 4.

More information

Setting a New Standard in Flash Chromatography Performance

Setting a New Standard in Flash Chromatography Performance Setting a New Standard in Flash Chromatography Performance What s New Faster Flow rates, up to 300 ml/min Higher pressures, up to 300 psi (20 bar) Bigger touchscreen, 12 or 15 inches Wider Dynamic Range

More information

Analysis of Benzenesulfonic Acid and P-Toluenesufonic Acid Esters in Genotox Monitoring using UPLC/UV-MS

Analysis of Benzenesulfonic Acid and P-Toluenesufonic Acid Esters in Genotox Monitoring using UPLC/UV-MS Analysis of Benzenesulfonic Acid and P-Toluenesufonic Acid Esters in Genotox Monitoring using UPLC/UV-MS Peter Alden and Michael Jones Waters Corporation, Milford, MA, U.S. APPLICATION BENEFITS UPLC combines

More information

Svensk läkemedelsstandard

Svensk läkemedelsstandard Svensk läkemedelsstandard 2018.2 Nitrogen Postadress/Postal address: P.O. Box 26, SE-751 03 Uppsala, SWEDEN Besöksadress/Visiting address: Dag Hammarskjölds väg 42, Uppsala Telefon/Phone: +46 (0)18 17

More information

Fungi-Plex Kit HOW TO USE IT F E C C. Wash Buffer [F] Standard Diluent Buffer [E] Assay Diluent Buffer [D] Mycotoxin Standard Mix

Fungi-Plex Kit HOW TO USE IT F E C C. Wash Buffer [F] Standard Diluent Buffer [E] Assay Diluent Buffer [D] Mycotoxin Standard Mix TM ungi-plex Kit W T U IT tandard iluent uffer [] Mycotoxin tandard Mix ssay iluent uffer [] etection Reagent ead Mix t i K x Wash uffer [] TY I T u U e h T I I I V Y PR I Y R T Y M T Y W T I T R 9 9 P

More information

FRANZ CELL TEST OF NANO GLUTATHIONE WITH HPLC ANALYSIS

FRANZ CELL TEST OF NANO GLUTATHIONE WITH HPLC ANALYSIS FRANZ CELL TEST OF NANO GLUTATHIONE WITH HPLC ANALYSIS Analysis Conducted BY CC RESEARCH (P) Ltd., For Nanoceutical Solutions Inc. USA 2950 Thousand Oaks drive, Suite 3, San Antonio, Texas EXECUTIVE SUMMARY

More information

DISSOLUTION TEST FOR SOLID DOSAGE FORMS

DISSOLUTION TEST FOR SOLID DOSAGE FORMS Seite 1 von 15 01/2010:20903 corrected 6.8 2.9.3. DISSOLUTION TEST FOR SOLID DOSAGE FORMS This test is provided to determine compliance with the dissolution requirements for solid dosage forms administered

More information

Presence and metabolism of natural steroids in meat-producing animals: current knowledge and potential strategies for detecting their abuse

Presence and metabolism of natural steroids in meat-producing animals: current knowledge and potential strategies for detecting their abuse Presence and metabolism of natural steroids in meat-producing animals: current knowledge and potential strategies for detecting their abuse James Scarth, HFL, UK October 2007 Overview of presentation Context

More information

CHE 4115 Chemical Processes Laboratory 2 Experiment 1. Batch Distillation

CHE 4115 Chemical Processes Laboratory 2 Experiment 1. Batch Distillation CHE 4115 Chemical Processes Laboratory 2 Experiment 1 Batch Distillation BACKGROUND Distillation is one of the most commonly used unit operations in chemical engineering. In general, a distillation operation

More information

Gradients in ion chromatography. Optimal separation with shorter analysis time

Gradients in ion chromatography. Optimal separation with shorter analysis time Gradients in ion chromatography Optimal separation with shorter analysis time Gradients yield precise results faster 02 The goal of ion chromatography in a nutshell reads: optimum separation within an

More information

Sensitive Analysis of Genotoxins by HPLC-ECD Using Boron-Doped Diamond Electrochemical Cell

Sensitive Analysis of Genotoxins by HPLC-ECD Using Boron-Doped Diamond Electrochemical Cell Sensitive Analysis of Genotoxins by HPLC-ECD Using Boron-Doped Diamond Electrochemical Cell Bruce Bailey, Marc Plante, Christopher Crafts, Paul Gamache, John Waraska, and Ian Acworth ESA A Dionex Company,

More information

2011 PROHIBITED DRUG CLASSES AND METHODS. Dr Nicolas Theron Loch Logan Waterfront Sport and Travel Medicine Centre Tel :

2011 PROHIBITED DRUG CLASSES AND METHODS. Dr Nicolas Theron Loch Logan Waterfront Sport and Travel Medicine Centre Tel : 2011 PROHIBITED DRUG CLASSES AND METHODS Dr Nicolas Theron Loch Logan Waterfront Sport and Travel Medicine Centre Tel : 051-4481389 Doping is defined as the administration of substances belonging to prohibited

More information

RayBio Human vwf ELISA Kit

RayBio Human vwf ELISA Kit RayBio Human vwf ELISA Kit Catalog #: ELH-vWF User Manual Last revised April 15, 2016 Caution: Extraordinarily useful information enclosed ISO 13485 Certified 3607 Parkway Lane, Suite 100 Norcross, GA

More information

MSD 96-Well MULTI-ARRAY CRP Assay

MSD 96-Well MULTI-ARRAY CRP Assay MSD 96-Well MULTI-ARRAY CRP Assay The following assay protocol has been optimized for analysis of C-reactive protein (CRP) in human serum and plasma samples. MSD Materials Storage Read Buffer T (4X), with

More information

Introduction to the Doping Problem

Introduction to the Doping Problem Introduction to the Doping Problem Jordi Segura Director, WADA Accredited Antidoping Laboratory, IMIM-Hospital del Mar, Barcelona, Spain Doping and Society: towards the perfect human machine? ESOF, Barcelona

More information

Alkylphenol Contamination in Homarus americanus

Alkylphenol Contamination in Homarus americanus University of Connecticut DigitalCommons@UConn Honors Scholar Theses Honors Scholar Program Spring 5-9-2010 Alkylphenol Contamination in Homarus americanus Jennifer Renee Urban University of Connecticut

More information

Carrier Gases in Capillary GC

Carrier Gases in Capillary GC Carrier Gases in Capillary GC LC Columns and Consumables Mark Sinnott Application Engineer January 15, 2009 CARRIER GAS Mobile Phase Carries the solutes down the column Selection and velocity influences

More information

Optimizing Vial Pressurization Parameters for the Analysis of <USP 467> Residual Solvents Using the 7697A Headspace Sampler

Optimizing Vial Pressurization Parameters for the Analysis of <USP 467> Residual Solvents Using the 7697A Headspace Sampler Optimizing Vial Pressurization Parameters for the Analysis of Residual Solvents Using the 7697A Headspace Sampler Application Note Pharmaceuticals Author Roger L Firor Agilent Technologies, Inc.

More information

GROWTH PROMOTERS Chapter 5

GROWTH PROMOTERS Chapter 5 GROWTH PROMOTERS Chapter 69 Growth Promoters b-agonists ANTIBODIES TRACER SPECIFICITY IMMUNOGEN Unit* Cat. No. Tracer Description Unit Cat. No. CIMATEROL Cimaterol-BSA 1ml PAS9848 Cimaterol-HRP 0.ml HRP9410

More information

EFFECTS OF REVIVOGEN SCALP THERAPY ON TESTOSTERONE METABOLISM IN RECONSTRUCTED HUMAN EPIDERMIS

EFFECTS OF REVIVOGEN SCALP THERAPY ON TESTOSTERONE METABOLISM IN RECONSTRUCTED HUMAN EPIDERMIS IN VITRO BIOLOGICAL TESTING BIOalternatives The state-of-the-art laboratory Proposal n : AD070315C-2 Study n : AD070315B EFFECTS OF REVIVOGEN SCALP THERAPY ON TESTOSTERONE METABOLISM IN RECONSTRUCTED HUMAN

More information

International Journal of Research in Pharmaceutical and Nano Sciences Journal homepage:

International Journal of Research in Pharmaceutical and Nano Sciences Journal homepage: Research Article CODEN: IJRPJK ISSN: 2319 9563 International Journal of Research in Pharmaceutical and Nano Sciences Journal homepage: www.ijrpns.com SIMULTANEOUS ESTIMATION AND VALIDATION OF TAMSULOSIN

More information

AKTA ION EXCHANGE CHROMATOGRAPHY SOP Date: 2/02/05 Author: A DeGiovanni Edited by: C. Huang Reviewed by:

AKTA ION EXCHANGE CHROMATOGRAPHY SOP Date: 2/02/05 Author: A DeGiovanni Edited by: C. Huang Reviewed by: 1 AKTA ION EXCHANGE CHROMATOGRAPHY SOP Date: 2/02/05 Author: A DeGiovanni Edited by: C. Huang Reviewed by: Materials/Reagents/Equipment Vendor 1. 0.2 um filtered Water + 0.05% sodium azide 2. 0.2 um filtered

More information

DETERMINATION OF TETRAHYDROTHIOPHENE IN AMBIENT AIR BY GAS CHROMATOGRAPHY WITH A PFPD DETECTOR COUPLED TO A PRECONCENTRATION TECHNOLOGY

DETERMINATION OF TETRAHYDROTHIOPHENE IN AMBIENT AIR BY GAS CHROMATOGRAPHY WITH A PFPD DETECTOR COUPLED TO A PRECONCENTRATION TECHNOLOGY DETERMINATION OF TETRAHYDROTHIOPHENE IN AMBIENT AIR BY GAS CHROMATOGRAPHY WITH A PFPD DETECTOR COUPLED TO A PRECONCENTRATION TECHNOLOGY Nengbing Xu, Hongmei Ying and Libo Zhu Ningbo Environmental Monitoring

More information

The instrument will process the samples one by one till all the samples have been cleaned up.

The instrument will process the samples one by one till all the samples have been cleaned up. Table of Contents SPE-01 Cleanup Station... 1 LC-04SP Valve System... 5 LC-04SP Standalone Valve... 10 LC-05 Auto Injector... 12 LC-06 Dosing Pump... 16 LC-08 Column Selector... 17 SPE-01 Cleanup Station

More information

Use of biotechnology to improve muscle growth in aquaculture species: Preliminary results on the use of myostatin in tilapia

Use of biotechnology to improve muscle growth in aquaculture species: Preliminary results on the use of myostatin in tilapia Nov. 12, 2011 HAAA Workshop Use of biotechnology to improve muscle growth in aquaculture species: Preliminary results on the use of myostatin in tilapia Yong Soo Kim, PhD Department of Human Nutrition,

More information

N Korea Japan China Thailand Taiwan Philipines EP-5 EP km. Source: Google Maps and

N Korea Japan China Thailand Taiwan Philipines EP-5 EP km. Source: Google Maps and OCCURRENCES AND TRANSPORT OF PERFLUORINATED COMPOUNDS IN EAST CHINA SEA Kunacheva C 1, Fujii S 1, Tanaka S 1, Shimizu J 2 and Shivakoti B R 1 1 Graduate School of Global Environmental Studies, Kyoto University,

More information

Prep LC Training Manual

Prep LC Training Manual Prep LC Training Manual (11-6-2013) Location: 1238 Hach Hall Contacts: kamel Harrata and Steve Veysey, 1234 Hach Hall Safety: Introduction: The Agilent PrepStar SD-1 preparative HPLC is a student operated

More information

GUIDE TO ULTRA-FAST HPLC. Quick Tips for Converting Conventional Reversed-Phase HPLC Separations to Ultra-Fast Separations

GUIDE TO ULTRA-FAST HPLC. Quick Tips for Converting Conventional Reversed-Phase HPLC Separations to Ultra-Fast Separations GUIDE TO ULTRA-FAST HPLC Quick Tips for Converting Conventional Reversed-Phase HPLC Separations to Ultra-Fast Separations GUIDE TO ULTRA-FAST HPLC Quick Tips for Converting Conventional Reversed-Phase

More information

DOS in Food Science & Nutrition, Manasagangotri, Mysore

DOS in Food Science & Nutrition, Manasagangotri, Mysore Sl No UNIVERSITY OF MYSORE DOS in Food Manasagangotri, Mysore 570 006. TENDERS FOR THE SUPPLY OF EQUIPMENTS, NETWORKING & COMPUTATIONAL FACILITIES FOR UNIVERSITY OF MYSORE (UNDER UGC XI SCHEME) INVITATION

More information

AKTA MC SOP Page 1 9/27/04 AKTA METAL CHELATING SOP

AKTA MC SOP Page 1 9/27/04 AKTA METAL CHELATING SOP AKTA MC SOP Page 1 9/27/04 Date: 9/27/04 Author: A DeGiovanni Edited by: R Kim Reviewed by: Y. Lou AKTA METAL CHELATING SOP Materials/Reagents/Equipment Vendor 1. Water + 0.05% sodium azide 2. 0.2 um filtered

More information

Prohibited substances in sport supplements

Prohibited substances in sport supplements Prohibited substances in sport supplements International Conference on Doping and Public Health, Oslo, Norway Olivier de Hon Introduction Supplements & Sport; a topic for several millennia Ancient Olympic

More information

PURE PERFORMANCE IN SPORT: ANTI-DOPING

PURE PERFORMANCE IN SPORT: ANTI-DOPING PURE PERFORMANCE IN SPORT: ANTI-DOPING A presentation by AFL Victoria ASADA 2012. This document is dynamic and subject to change. Please refer to ASADA e-learning to ensure use of the current version.

More information

UWW ANTI-DOPING PANEL DECISION. Case

UWW ANTI-DOPING PANEL DECISION. Case UWW ANTI-DOPING PANEL DECISION Case United World Wrestling (UWW) v. Mr Dmitrii Elkanov (Athlete Freestyle Wrestling member of the Russian cadets national team) Panel: - Dr Daniel Wozniak - Dr Milica Vukasinovic-Vesic

More information

DSC 204 HP Phoenix. High-Pressure Differential Scanning Calorimetry up to 15 MPa Method, Technique and Applications

DSC 204 HP Phoenix. High-Pressure Differential Scanning Calorimetry up to 15 MPa Method, Technique and Applications DSC 204 HP Phoenix High-Pressure Differential Scanning Calorimetry up to 15 MPa Method, Technique and Applications DSC 204 HP Phoenix The ability to apply pressure improves the capabilities of Differential

More information

AKTA pure 25 New Owner s Intro

AKTA pure 25 New Owner s Intro AKTA pure 25 New Owner s Intro The exercise below will give a quick demonstration of how easy and intuitive the AKTA pure 25 will be for you in demonstrating downstream processing to your students. Steps

More information

Operation of the Perkin Elmer TGA-GC/MS

Operation of the Perkin Elmer TGA-GC/MS Operation of the Perkin Elmer TGA-GC/MS Summary of the TGA-GC/MS: The TGA-GC/MS allows a user to decompose a sample by heating, measure its loss of mass, and simultaneously analyze the chemical composition

More information

BCAC ANTI DOPING POLICY

BCAC ANTI DOPING POLICY BCAC ANTI DOPING POLICY Version 1.5 May 14, 2014 ARTICLE 1 - DEFINITION OF DOPING For the purposes of this document, doping is defined as the occurrence of one (1) or more of the anti-doping policy contraventions

More information

61D Permitted Medications for Horses. (1) The prescription medications defined in this rule shall be permitted under the conditions set forth

61D Permitted Medications for Horses. (1) The prescription medications defined in this rule shall be permitted under the conditions set forth 61D-6.008 Permitted Medications for Horses. (1) The prescription medications defined in this rule shall be permitted under the conditions set forth to conserve and protect the health of the horse which

More information

Updates on Anti-doping and TUE Management in Paralympic Sport

Updates on Anti-doping and TUE Management in Paralympic Sport International Paralympic Committee Updates on Anti-doping and TUE Management in Paralympic Sport Matthew Fedoruk, Ph.D. March 15, 2018 PyeongChang 2018 IPC Medical / Sports Science Committee Workshops

More information

CORESTA RECOMMENDED METHOD Nº 67

CORESTA RECOMMENDED METHOD Nº 67 CORESTA RECOMMENDED METHOD Nº 67 DETERMINATION OF WATER IN THE MAINSTREAM SMOKE OF CIGARS BY GAS CHROMATOGRAPHIC ANALYSIS (November 2005) 1. FIELD OF APPLICATION The method is applicable to the particulate

More information